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Reprosil Chiral-CA is a so called brush-type phase like the other chiral Reprosil phases:
-Reprosil Chiral-NR: for Normal- and Reversed Phase separations with a very broad
generality.
-Reprosil Chiral-OH: for aromatic compounds with an OH-group on the chiral centre.
-Reprosil Chiral-PS: for aromatic compounds, which contain a S or P atom.
-Reprosil Chiral-AA: for all Amino Acids and Oxazolidinones, Hydantoins, Diazepines and Sulfoxides.
Most successfully separated compounds are:
1.) are aromatic,
2.) carry a carboxylic acid group on the chiral centre and
3.) are less hydrophilic than Amino Acids, which can not be separated without modification.
A good example is the separation of Ibuprofen.
Due to the 100A° pores and the big surface area of 350 m2/g the phase has an excellent preparative capacity. With a 250 x 10 mm column one can separate 50 – 250 mg / injection and with a 250 x 20 mm column 250 – 1000 mg/ injection.
The phase is stable in all commonly used NP eluents. Typical eluents are mixtures of Hexane / tert-Butylmethyl-Ether or Hexane and Isopropanol.
The best pH-range is between 2 und 7. The columns are stable up to 300 bar.
Examples for separations:
The typical column dimension is 250 x 4.6 mm with a flow of 2 ml / min.
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Eluents for Carboxylic-Acids: |
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Benoxaprofen: |
Eluent: Hexane / tert-Butylmethyl Ether / Acetic Acid ( 60/40/01.) |
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Carprofen: |
Eluent: tert-Butylmethyl Ether / Acetic acid (100 / 0.1) |
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2-(4-Chlorophenoxy) propionic Acid: |
Heptane/tert-Butylmethyl Ether/Formic Acid (70/30/0.1) |
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Etodolac: |
Eluent: Hexane / tert-Butylmethyl-Ether / Acetic Acid (75 / 25 / 0.1) |
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Flurbiprofen: |
Eluent: Hexane / tert-Butylmethyl-Ether / Acetic Acid (60 / 40 / 0.1) |
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Ibuprofen: |
Eluent: Hexane / tert-Butylmethyl Ether / Acetic Acid (75 / 25 / 0.1) |
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Ketoprofen: |
Eluent: Hexane / tert-Butylmethyl Ether / Acetic Acid (60 / 40 / 0.1) |
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a-Methoxyphenylacetic Acid: |
Hexane / tert-Butylmethyl Ether / Acetic Acid (85 / 15 / 0.1) |
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Naproxen: |
Eluent: Hexane / tert-Butylmethyl Ether / Acetic Acid (60 / 40 / 0.1) |
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Pirprofen: |
Eluent: Hexane / tert-Butylmethyl Ether / Acetic Acid (60/40/0.1) |
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Eluents for racemates with a Carbonyl-Group at or near by the chiral centre: |
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Acenocoumarol: |
Hexane / 2-Propanol (93 / 7) + 0.1% Acetic acid |
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Baclophenlactam: |
Hexane / 2-Propanol (95 / 5) |
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Bucetin: |
Hexane / 2-Propanol (97 / 3) |
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Bupivacain: |
Hexane / 2-Propanol / Essigsäure / Triethylamin (98 / 1/ 0.3 / 0.05) |
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Camazepam: |
Hexane / tert-Butyl-Methyl-Ether / 2-Propanol (80 / 20 / 1) |
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Carticain: |
Hexane / 2-Propanol / Essigsäure / Triethylamin (98 / 1/ 0.3 / 0.05) |
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p-Chlorophenprocoumon: |
Hexane / 2-Propanol / tert-Butyl-Methyl-Ether (65/5/30) + 0.3% Acetic acid |
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Lopirazepam: |
Hexane / tert-Butyl-Methyl-Ether / 2-Propanol (50 / 40 / 10) |
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Lorazepam: |
Hexane / tert-Butyl-Methyl-Ether / 2-Propanol (50 / 40 / 10) |
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Oxazepam: |
Hexane / 2-Propanol (85 / 15) |
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2-Phenoxy-Propanamid: |
Hexane / 2-Propanol (98 / 2) |
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Phenprocoumon: |
Hexane / 2-Propanol / tert-Butyl-Methyl-Ether (65/5/50) +0.3% Acetic acid |
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Tropicamid: |
Hexane / Tetrahydrofuran (80 / 20) |
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Omeprazole |
Hexane / 2-Propanol / Triethylamine / Acetic acid ( 92 / 8 / 0,15 / 0,5) |
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Method development for Normal-Phase Separations:
1.) Start off with a mixture of Hexane / IPA or Hexane / tert-Butylmethylether (70/30).
2.) If the RT is too short, add less IPA ( tert-Butylmethylether); if the RT is too long, add more.
3.) Peak-Tailing
with acids: use 0,1 % Acetic acid (or formic acid)
with bases: use 0,1 % TEA.
You can improve the peak shapes in some cases with Acetic acid together with TEA.
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Examples: Reprosil Chiral-CA, 5 µm, 250 x 4.6 mm, Part.No.: r15.ca.s2546 |
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